反应详情

58 mg of (1H-benzotriazol-1-yloxy)[tris(dimethylamino)]phosphonium hexafluorophosphate (BOP), 18 mg of hydroxybenzotriazole (HOBT), 9 mg of ammonium chloride and 0.07 ml of diisopropylethylamine are successively added to a solution of 40 mg of 4-[4-(6-cyanopyridin-3-yl)-9H-carbazol-9-yl]-2-[(2-fluoroethyl)amino]benzoic acid in 30 ml of N,N-dimethylformamide. The reaction mixture is stirred at ambient temperature for 2 hours and then diluted with distilled water and extracted with ethyl acetate. The organic phase is subsequently washed with distilled water and a saturated solution of sodium chloride, dried over magnesium sulphate, filtered and concentrated under reduced pressure. The residue is purified by silica gel chromatography, elution being carried out with a mixture of dichloromethane, acetonitrile and methanol (96/2/2 by volume), so as to gve 30 mg of 4-[4-(6-cyanopyridin-3-yl)-9H-carbazol-9-yl]-2-[(2-fluoroethyl)amino]benzamide in the form of a white solid, the characteristics of which are the following:

1. extractionextracted with ethyl acetate
2. washThe organic phase is subsequently washed with distilled water
3. dry with materiala saturated solution of sodium chloride, dried over magnesium sulphate
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe residue is purified by silica gel chromatography, elution
7. additionbeing carried out with a mixture of dichloromethane, acetonitrile and methanol (96/2/2 by volume)